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Ammonium Hydroxide → (R)-quinuclidin-3-yl 2-amino-2-phenylacetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | (R)-Quinuclidin-3-yl 2-amino-2-phenylacetate dihydrochloride | HCID 67425463 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | (R)-quinuclidin-3-yl 2-amino-2-phenylacetate | HCID 59401091 | 73.2% |
反応手順
(R)-Quinuclidin-3-yl 2-amino-2-phenylacetate dihydrochloride (C25) (1.11 g, 3.33 mmol) is dissolved in MeOH (10 mL) and 32% NH4OH (2.0 mL, 16.07 mmol) is added. The solution is stirred at RT for 30 seconds and then is evaporated under vacuum. The residue is dissolved in DCM/MeOH (4.5/0.5 mL) and about 1 g of SiO2 is added. The suspension is evaporated and the residue is loaded on a silica gel column and purified eluting with DCM/MeOH/NH4OH=9.2/0.8/0.1 to 9/1/0.1 to collect intermediate I124 as a pale yellow oil (635 mg, 73% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08835682B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-434a3f9a2b874354904a9966d7e4c671 |
| 出典メモ | uspto-grants-2014_09 |